Synthesis Of Alkylcyclophosphanes From Red Phosphorus - Molecular Structure Of I-Pr4p4 By Gas Electron Diffraction

A polyphosphide of the type (NaP)(x) 1 was obtained from red phosphorus and sodium in presence of small amounts of naphthalene in 1,2-dimethoxyethane as solvent. 1 reacts with alkyl halides in dependence on the kind of alkyl group with formation of different alkylcyclophosphanes. As definite compounds Me5P5 2, Et5P5 3 (With not definite constitution), i-Pr4P4 4 and t-Eu4P4 5 could be isolated.1 was identified by X-ray diffraction, 2-5 by means of their H-1, C-13, P-31 n.m.r. and mass spectra. The molecular structure of 4 was identified by electron diffraction.